|
First, the purpose of the kidney complex Granules quantitative fingerprinting and in vitro dissolution study in order to achieve better control of renal complex Granules quality and uniformity of purpose. Method 1. Determination of 1.1 using Agilent TC-C18 column (4.6 mm × 250 mm, 5 μm); mobile phase: 0.05% phosphoric acid: acetonitrile (95:5); flow rate: 1 mL / min, detection wavelength 273 nm, which was not gallic acid content the kidney complex Shu particles. 1.2 using the Agilent TC-C18 column (4.6 mm × 250 mm, 5μm), methanol and 0.1% glacial acetic acid as the mobile phase gradient elution (0-20 min, methanol from 40% -60%, 0.1% glacial acetic acid 60% -40%; 20-40 min, methanol from 60% -85%, 0.1% glacial acetic acid by 40% -15%; 40-45 min, 85% methanol, 0.1% glacial acetic acid 15%), flow rate: 1.0 ml / min, λ1 = 276 nm (seized glycyrrhizin), λ2 = 283 nm (seized naringin), λ3 = 254 nm (check Chrysophanol), column temperature: 30 ° C, simultaneous determination of renal complex the comfortable particles (rhubarb licorice and trifoliate) in Chrysophanol, licorice and naringin content. Fingerprinting using a diode array detector, the kidney complex Shu particles, each with 12 batches, to the volume fraction of 50% alcohol solution of methanol ultrasonic extraction preparation solution, the application of Agilent TC-C18 column (4.6mm × 250 mm, 5μm), to 0.05 % phosphoric acid and acetonitrile as the mobile phase gradient elution with a flow rate of 1mL · min-1, column temperature of 30 ° C and the detection wavelength was 254 nm. Dissolution studies in order to effectively control the quality of the goods, the goods in vitro dissolution studies. 0.1mol / L hydrochloric acid solution 500 mL dissolution medium slurry method 100r/min, visits the kidney complex Shu particle release from chrysophanol, licorice and naringin in vitro dissolution. Results 1 Determination of Gallic sub-acid 11.60μg/mL-116.00μg/mL peak area showed a good linear relationship (r = 1), recoveries (n = 6) were 99.9%, RSD 0.46%; chrysophanol 6.82μg/mL ~ 136.4μg/mL and peak area showed good linear relationship (r = 0.9999), naringin 5.52 ~ 82.8μg/mL was a good linear relationship with the peak area, r = 0.9999, liquiritin 17.52 ~ 175.2μg/mL was a good linear relationship with the peak area, r == 1. The average recoveries (n = 9): the chrysophanol of 99.5%, the naringin 99.4%, glycyrrhizin 99.5%; measured gallic acid content: 1.55 mg / g, the chrysophanol 0.36mg / g glycyrrhizin 3.53 mg / g, the Naringin 1.90 mg / g. Fingerprints kidney complex Granules extracts were detected a total of peaks, can identify 39 common peaks State Pharmacopoeia Commission fingerprint processing system (2004A), similarity of 12 batches of particles greater than 0.90. 3 the dissolution studies 45min Kidney the complex The Shu particles dissolution results were, the chrysophanol 86.7% (RSD = 1.6%), 86.3% (RSD = 1.6%), 85.7% (RSD = 2.3%); glycyrrhizin 88.9% (RSD = 1.2%), 87.2% (RSD = 1.2%), 86.9% (RSD = 1.7%); the naringin 86.4% (RSD = 1.1%), 87.4% (RSD = 1.3%), 85.3% (RSD = 1.5% ). , The kidney complex Granules conclusions of a study to determine the quantitative method is simple, reliable results, good reproducibility and can be used as the method of quality control of the product. 2 kidney complex Shu particles fingerprint research method is simple, stable, and good reproducibility. Applicable in the kidney complex Granules fingerprint detection. The experiment proved the strong kidney complex Shu particle dissolution exclusive, simple and feasible.
|